Manufacture of linoleum and the like



ALFRED BREWERTON CRAVEN, or SELBY, ENGL'ANR; nssrenon; BY mnsun assren- MENTS, T0 YORKSHIRE DYEWARE a CHEMICAL COMPANY LI ITE or LEEDS,

I YORK, ENGLAND. 7

MANUF CTURE or LINOLEUM AND THE LIKE.

No Drawing.

To all whom it may aoncermfi Be it known that I, ALFRED BREWERTON CRAVE-N, subject of the King of Great Britain, residing at Selby, Yorkshire, in the Kingdo-mof England, have invented certain new and useful Improvements in and Relating to the Manufacture of Linoleum and the like, of which the following is a specification. I

The resent invention relates to improvements 1n the manufacture of linoleum consisting in the use of a new material for this purpose and the invention is also designed to utilize more effectively certain by-products obtained in the oil manufacturing industry.

The by-products I employ are those consisting of liquid or semi-solid mixtures of fatty acids and glycerides in varying proportions and mucilage and colouring matter obtained in refining for edible and other purposes drying and/or partially drying oils. The refining operations which yield the byproducts I use are those generally in use'and consists of, for example: (a) Treatment of crude oil with a small quantity of strong soda lye sufficient to combinewith the free fatty acids present and to leave a slight excess of caustic soda, agitatingwell and warming gently then allowing to stand,

when the soap formed settles to the bottom it colouring matter products so that they contain'only those carrying down with mucilage and some of the Oll itself. The

clear refined oil is run off and, leaves the foots as by-product which I acidify with mineral acid to convert the soap into fatty acids, and wash to remove mineral acid and its salt. (6) Refining by acid treatment which consists of heating and agitating the crude oil with a small amount of slightly diluted sulphuric acid and allowing to stand. When the clear oil is run off, the sediment consisting of mucilage and oil is a suitable by-product after being washed free from mineral acid. (0) Similar sediments resulting from other processes of refining such as treatment with bichromate of potash and mineral acid, and any sediment formed when a partly refined drying or partially drying oil, or boiled oil is allowed to stand in a tank, are all suit-able for my process. (at) The oily matter absorbed bv fullers earth which has been used in refining is also suitable when extracted from the fullers earth by a volatile solvent or by other means.

Application filed October 31 1913. Serial No. 260,585.

I could use the commercial drying oils and/ or partly drying oils or mixtures of these oils and their fatty acids, .or their commercial fatty acids, but I prefer to'make use of the by-products above mentioned as the most economical source of my raw materials.

The new material I use for the manufacture of linoleum is the resilient tacky and adhesive residue obtained from the distillation of the aforesaid by-products. The foots' and waste products from the 'oil manufacturing industry are usually worked up by. distillation and the main object is to obtain commercially'usable fatty acids as a distillate. The residue left in the still at the end of this operation'usually consists of black pitch which is of low'commercial value.

. This by-produ ct of distillation (the resii due) is usually quite unsuitable for use in the manufacture of linoleum. I have found,

however, that whereas the foots from non-' drying oils and fats on distillation yield dark non-resilient andbrittle residues which are unsuitable for linoleum manufacture that on the contrary-those from drying oils and/or partially drying oils,'or mixtures largely consisting thereof, can be distilled in such manner 'as to yield a product which is very valuable for use in making a cement for linoleum manufacture. According to' the present invention I keep separate the waste from the. drying oils or partially drying oils 4 and a re'free from the products of non-dry ing oils and I distil them with the definite object of obtaining a product which will be The distillation is to be conducted in such 7 manner and stopped at such a stage that a large yield is obtained of a residue which'is/ resilient, adhesive. and showing maximum paleness of colour and freedom 'from smell, I

by virtue of which qualities the product'becomes suitable for linoleum manufacture.

' The by-products fromdrying oils may be distilled without mixture with by-products from partly-drying oils, or the latter bye products may be distilled without mixture with drying oil by-products, or the byproducts from drying oils and partly-drying oils may be mixed and distilled together, but I do not mix any by-products of non-drying oils with those of the other classes but ensure the absence ofnon-drying oil by-products by having them kept separate in the works where they are made. The distillation of by-products from drying and partly-drying oils without any non-drying o-il by-products drying oils and partially drying oils by 5 thickening the. oil by-products "and this thii-kenina may-be'efi'ected by heating before the distillation commences. W

The distillation process removes from the fatty matter certain solid saturated fatty bodies which are detrimental for my pur- .o e.- 1. e, myr s ic, palmitic and stearic acids and also the fluid unsaturated oleic. acid which, is also detrimental. The more unsaturated acids '(linolic', clupa-nodonic and flinolenic) and their glycerides becomethickened or ploymerized. The-heat is supplied 7 by afire under'the still and the temperature may reach 300 degrees C.', and the heat is maintained until a decided thickening, due

to polymerization of the more unsaturated bodies has taken place. During distillation, thickening also takes place, due to polymerization, and also due to the removal of non-thickening bodies, and leavesbehind, when stopped at the right stage,.the resilient,'tacky and adhesive mass.

The paleness and freedom from smell are improved-by rigid exclusion of. air during thickeningandduring distillation,-e. g-.,' by

- working in an airtight-still in vacuo, or 1n presence of an inert gas, e. g., carbon dioxide or by superheated steam or'by a combination of these methods. The waste-fatty products may be treated by any known method in order to remove foreign -matter and fatand improve the colour before sub-- mission to the thickening and. distillation. The colour of the by-products may be im proved or bleached by heating with a solu- .tion of. bleaching powder and then adding mineral acid and-washing free from mineral acid. Or by washing with strong alkaline lye, which dissolves the colour and also forms soap-which is almost insoluble in the strong lye. The coloured lye is run away from the soap and the soap decomposed with istics.

suitable for ture.

mineral acid and the paler oil product is washed.

The filtration of the by-pro'ducts may be done in a filter press when the by-products are pumped in and a pressure maintained to hasten the operation and toyield a cake of fatty matter and foreign matter of some firmness which may be further pressed in a hydraulic press to yield more clear oil products. The clear portion from both these operations is distilled. The removal of the solid fat reduces the time required for the production of the residue, because the bodies which produce the particular residue I make, are liquid at ordinary temperatures, and any solid fat introduced into the still must be removed by the distillation before the residue can have the required character- Other known methods of bleaching andremoval of solid bodies may be used with the same object.

Eaqample.

matter, by washingwith strong alkaline lye or other suitable means, and decomposing the soap withmineral acid and washing free from mineral acid. Thirty cwts. of the product are charged into a still made of cast iron provided with a safety valve and arranged to be heated by fire. The air is exhausted and then the still is closed airtight. The fire is started and the temperature raised to 270 to 300 degrees (1., and

maintained thereat for 1 to 2 hours, any

matter in the still andthe temperature isregulated to give a steady delivery of pale fatty acid distillate and water. This distilling is continued until the residue left in the still is non-greasy and when cold, resilient, tacky and adhesive. This residue is then run out, and may be used for the manufacture of linoleum and the like.

The product/may be used in the usual way by incorporating it with cork or wood fibre and pigments so as to form linoleum,'or it may be used in conjunction with linoleum cement made from linseed oil or the like for the manufacture of linoleum or other material. -The product itself may also be used ,forfthe other known purposes for which linoleum cement made from linseed oil is suitable. During or after the manufacture of thep-roduct gum resin, or other bodies may be added to the product to'make it more purposes of linoleum manufac- I declare that what I claim is 1. The process of obtaining an agglutinant for the manufacture of linoleum which consists in submitting to a distilling temperature, out of contact with free oxygen substances containing the radical of an unsaturated acid more unsaturated than oleic acid, and of the kind occurring in more or less drying oils, until the residue goes beyond the varnish stage and becomes semisolid, resilient, tacky and adhesive :the ag glutinant aforesaid.

2. The process of obtaining an agglutinant for the manufacture of linoleum consisting of submitting oils of a more or less drying character to a distilling temperature out of contact with free oxygen when the non-drying portion of .the oils distils over and the residue goes beyond the varnish stage and becomes semi-solid resilient tacky and adhesive-the agglutinant aforesaid.

3. The process of obtaining an agglutinant for the manufacture of linoleum consisting of submitting a mixture of more or less drying oils and their fatty acids to a distilling temperature out of contact with free oxygen when the non-drying portion of the mixture distils over and the residuegoes beyond the varnish stage and becomes semi-solid resilient. tacky and adhesive.

4. The process of obtaining an aggluture of linoleum consisting of submitting of these by-products distils over and the residue goes beyond the varnish stage and becomes semi-solid, resilient, tacky, and adhesive.

tinant for the manufacture of linoleum con 1 sisting of distilling substances containing the radical of a fatty acid more unsaturated than oleic acid in a current of'superheated steam to assist in the removal of non-drying matter therefrom from any of the materials mentioned in claim 1. i i

7'. The process of obtaining an agglutinant for linoleum containing the purificationresidue from by-products from more or less drying oils which consists of submitting the said by-products to a preliminary filtration and then submitting them to a distilling temperature out of contact with free oxygen;

8. That step in the process of obtaining an agglutinant for linoleum from the ma terials as set forth in claim 1, which'con sists in bleachingthe said materials before the distillation operation, with the object of producing a paler agglutinant.

9. The process of obtaining an agglutin ant for linoleum from the materials mentioned in claim 1, which consists in first submitting the said materials to a preliminary heating for a prolonged period as described out of contact with free oxygen whereby the oil is polymerized and then submitting the materials to a distilling temperature out of contact with free oxygen.

10. As a new article of manufacture a semi-solid tacky and adhesive distillation residue for mixing with powdered cork and the like,'for making linoleum which consists of the bodies mentioned in claim 1 thickened and more or less polymerized beyond the varnish stage, such material being of a tacky and adhesive character and semi-solid at ordinary room temperature but substantially free from non-drying oil derivatives and consisting substantially of polymerized bodies derived from acids more unsaturated than oleic acid.

In witness whereof, I have hereunto signed my name this 8th day of October 1918, in the 'presence of two subscribing witnesses.

ALFRED BREWERTON CRAVEN.

Witnesses:

LUoY COSTIGAN, R. RAYMOND HAYNES. 

